布洛芬甲酯的绿色合成工艺  

Green Synthesis Process of Ibuprofen Methyl Ester

作　　者：曹雅晴[1] 汤鲁宏[1] 

机构地区：[1]江南大学药学院,江苏无锡214122

出　　处：《精细化工》2013年第1期56-60,98,共6页Fine Chemicals

基　　金：2011年度江苏省产学研联合创新资金(BY2011121)~~

摘　　要：以布洛芬和甲醇为原料,以对甲苯磺酸为催化剂,以甘油作为吸水剂和催化剂分离的溶剂,利用甘油与布洛芬甲酯可自动分层的特性,辅以柱色谱分离,建立了一种布洛芬甲酯的绿色合成工艺。整个工艺路线无三废产生。合成条件经正交实验优化,确定了最佳反应条件:反应体系的最佳组成为n(布洛芬):n(甲醇):n(甘油)=1:10.2:1.4,催化剂对甲苯磺酸的最佳添加量为布洛芬质量的1%,最佳转速为300 r/min,最佳反应时间为4h,在该条件下转化率可达97.1%,得率大于95.0%。经液相-质谱联用(LC/MS)检测,色谱纯度为99.9%。An environmentally benign process has been established for the production of ibuprofen methyl ester,with ibuprofen and methanol as reactants,p-toluene sulfonic acid（PTSA） as catalyst ,and glycerol as the adsorbent of water and the solvent of catalyst. The immiscibility of glycerol and ibuprofen methyl ester was exploited in this benign process. The chromatography was used to isolate the products. For the whole process, there was no discharge of effluent either during the process of synthesis or that of the purification. The reaction conditions have been optimized as follows： the optimal molar ratio of reactants was n （ ibuprofen ） ： n （methanol） ： n （glycerol） = 1 ： 10. 2：1.4 ; the optimal amount of PTSA was 1% of ibuprofen ;the optimal reaction time was 4 h; and the optimum stirring speed was 300 r/min. Under the optimized conditions, the conversion rate could reach 97. 1% , and the yield was more than 95%. Detected by LC/MS, the purity of ibuprofen methyl ester was 99.9%.

关 键 词：布洛芬 布洛芬甲酯 对甲苯磺酸 甘油 医药原料 

分 类 号：TQ463.4[化学工程—制药化工]